CN104233301A - Metallographic etchant used for HR-2 antihydrogen steel, and preparation method and corrosion method of metallographic etchant - Google Patents
Metallographic etchant used for HR-2 antihydrogen steel, and preparation method and corrosion method of metallographic etchant Download PDFInfo
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Abstract
The invention discloses a metallographic etchant used for HR-2 antihydrogen steel, and a preparation method and a corrosion method of the metallographic etchant, and belongs to the technical field of the metallographic etchant. The metallographic etchant comprises nitric acid, hydrochloric acid and distilled water at the volume ratio of 1:3:5. The corrosion method comprises the following steps: 1) polishing, burnishing, cleaning and drying an HR-2 antihydrogen steel sample; 2) using a degreasing cotton to dip the newly prepared metallographic etchant, taking the wetted degreasing cotton to repeatedly scrub the surface of the sample to be corroded till the surface is silver gray; 3) immediately soaking the sample processed in the step 2) into the newly prepared metallographic etchant until a bubble which covers the surface of the sample is yellow; 4) taking out the sample, washing and drying to obtain an HR-2 antihydrogen steel metallographic observation sample, and observing the corrosion effect under a metallographic microscope. The metallographic etchant is a regular chemical agent, is simple to prepare and free of pollution, and subboundary, twin-boundary, crystal-boundary and austenite structures and strain-induced martensite are quite obviously observed.
Description
Technical field
The invention belongs to metallographic etchant technical field, be specifically related to a kind of metallographic etchant for HR-2 resistant to hydrogen steel and caustic solution.
Background technology
In the engineering system fields such as petrochemical complex and oil and gas, core, Aeronautics and Astronautics, hydrogen embrittlement is the principal element causing parts and equipment premature failure always.Along with the development in the fields such as aviation, ocean, oil, nuclear industry and Chu Qing, the performance requriements for the high strength anti-hydrogen embrittlement alloy used under facing hydrogen environment is more and more higher.Resistant to hydrogen alloy refers to can resistant to hydrogen damage or the metallic substance of anti-hydrogen embrittlement, can use, also can be used for the lining material of hydrogenation reaction tank and manufacture storage hydrogen pressure container etc. as structured material under High Pressure Hydrogen (10 ~ 70MPa) condition.
HR-2 resistant to hydrogen steel take Fe-Cr-Ni as principal element, adds the alloying elements such as Mn, N, with the single-phase stable state austenitic stainless steel of nitrogen solution strengthening, when bearing static load under normal temperature or impact, martensitic transformation can occur, separate out a small amount of carbide simultaneously.HR-2 resistant to hydrogen steel has good mechanical behavior under high temperature, high temperature oxidation resistance, corrosion resistance, good toughness, processing performance and weldability, is widely used in the main equipment that the High Temperature High Pressure such as petrochemical complex, nuclear power, steam turbine cylinder, thermoelectricity contact with hydrogen or hydrogen blending agent.Hydrogen by absorption, penetrate into material, assembled by diffusion a certain regional area in a metal, cause material property to decline, generally show as that hydrogen deduced plasticity damage subtracts, hydrogen-induced crack, hydrogen-induced delayed failure etc., be i.e. so-called hydrogen embrittlement.HR-2 resistant to hydrogen steel, under arms in process, often need to observe the metallographic structure of material, and the service state of bonding properties test data to material detects, and its prerequisite is the display adopting suitable etching reagent to realize tissue.
Usual HR-2 resistant to hydrogen steel application oxalic acid or salpeter solution carry out electrolytic corrosion, although can carry out, require instrumentation, time-consuming and need electricity, operation is comparatively complicated, clearly can not reflect the content of each phase.Fig. 1 is by the metallographic after the oxalic acid solution electrolytic corrosion of 10% in document, although the single phase austenite in original structure can be shown, and can not the subgrain of the complete crystal grain of clear display and intra-die.Although the metallographic etching agent of austenitic stainless steel adopts iron trichloride, hydrochloric acid, water to prepare according to certain volume percent, or hydrochloric acid, nitric acid, water according to certain volume percent preparation, but how volume percent controls the key becoming corrosive fluid.With the dense chloroazotic acid wiping specimen surface of new preparation, the rapid blackening of specimen surface, at metallography microscope Microscopic observation erosional surface tissue, crystal grain presents black, and crystal boundary is but still unintelligible; With the light chloroazotic acid wiping specimen surface shelved for a long time, then cannot erode away complete crystal boundary clearly.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of metallographic etchant for HR-2 resistant to hydrogen steel and preparation method thereof and caustic solution, this metallographic etchant erosion effect is good, pollution-free, corrosion safety is slow, stability is strong, and compound method is quick, efficient; Caustic solution is effective, and corrosion process is steady, and after corrosion, sample tissue display effect is good, workable.
The present invention is achieved through the following technical solutions:
For a metallographic etchant for HR-2 resistant to hydrogen steel, the volume ratio of being pressed 1:3:5 by nitric acid, hydrochloric acid and distilled water is formulated.
For a compound method for the metallographic etchant of HR-2 resistant to hydrogen steel, measure nitric acid, hydrochloric acid and distilled water respectively according to the volume ratio of 1:3:5, first hydrochloric acid is dissolved in distilled water, then adds nitric acid, stir, obtain the metallographic etchant for HR-2 resistant to hydrogen steel.
An etching pit method for HR-2 resistant to hydrogen steel, comprises the following steps:
1) HR-2 resistant to hydrogen steel curved beam is carried out polish, polishing, clean and dry up process, make and treat corrosion sample;
2) absorbent cotton is dipped the metallographic etchant of new preparation, the absorbent cotton that taking-up soaks repeatedly wiping treats that corrosion sample surface to surface is silver gray;
3) by step 2) sample after process immerses in the metallographic etchant of new preparation, and the bubble that etch to specimen surface covers is in yellow; During immersion, the metallographicobservation face of sample is parallel with the liquid level of metallographic etchant, and sightingpiston upwards;
4), after being taken out by sample, through washing, drying, HR-2 resistant to hydrogen steel metallographic observation sample is obtained, at metallography microscope Microscopic observation corrosive effect;
Wherein, metallographic etchant is formulated by the volume ratio of 1:3:5 by nitric acid, hydrochloric acid and distilled water.
Step 1) described in polishing be polish with the water-proof abrasive paper of 400#, 600#, 800# and 1000# successively, and every polishing together all will eliminate polishing scratch and the abrasive dust that a procedure stays metallographicobservation face.
Step 1) described in polishing be carry out mechanical polishing with the metallographic lapping paste that granularity is 10W and 5W successively.
Step 1) described in cleaning be clean with distilled water and dehydrated alcohol successively.
Step 2) described in the time of wiping be repeatedly 7 ~ 12min.
Step 3) described in the etch time be 3 ~ 5min.
Step 3) described in metallographicobservation face and erosional surface at a distance of 10 ~ 20mm.
Step 4) described in washing be first use distilled water flushing, more repeatedly to rinse with dehydrated alcohol; Step 4) described in drying be with hair dryer by washing after sample dry up.
Compared with prior art, the present invention has following useful technique effect:
Metallographic etchant for HR-2 resistant to hydrogen steel disclosed by the invention, reasonable in design, be conventional chemical reagent, preparation is simple, erosion effect is good, pollution-free, there is austenite and martensitic stucture clearly in the sample tissue through corroding, there is the advantage that display effect is good, pollution-free, corrosion reaction is slowly stable.The etching pit liquid making method of HR-2 resistant to hydrogen steel of the present invention is simply rapid, is used while allocating, very convenient.
The etching pit method of HR-2 resistant to hydrogen steel disclosed by the invention, corrosive effect is good, and crystal boundary, twin boundary, subgrain boundary are clear, has good circulation ratio, can observe austenite structure and strain-induced martensite more significantly.
Accompanying drawing explanation
Fig. 1 is the HR-2 resistant to hydrogen steel microscopic structure figure of prior art report;
Fig. 2 is the HR-2 resistant to hydrogen steel original sample micro-organization chart of the embodiment of the present invention 1;
Fig. 3 is the HR-2 resistant to hydrogen steel tension specimen micro-organization chart of the embodiment of the present invention 2.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Metallographic etchant for HR-2 resistant to hydrogen steel disclosed by the invention, the volume ratio of being pressed 1:3:5 by nitric acid, hydrochloric acid and distilled water is formulated.Wherein, nitric acid is concentrated nitric acid, and hydrochloric acid is concentrated hydrochloric acid.
The invention discloses the compound method of the metallographic etchant for HR-2 resistant to hydrogen steel, concrete operations are:
Carry out in draughty stink cupboard, before preparation, put on mouth mask and rubber gloves, measure nitric acid, hydrochloric acid, distilled water with graduated cylinder according to the volume ratio of 1:3:5, first hydrochloric acid is dissolved in distilled water, add nitric acid again, stir gently with glass stick, be mixed with metallographic etchant.
The invention also discloses a kind of etching pit method of HR-2 resistant to hydrogen steel, comprise the following steps:
1) HR-2 resistant to hydrogen steel curved beam is carried out polish, polishing, clean and dry up process, make and treat corrosion sample;
Fine grinding is more first roughly ground during polishing, fine grinding observation is carried out successively with 400#, 600#, 800#, 1000# water-proof abrasive paper, every one fine grinding all will eliminate the polishing scratch that a procedure stays sightingpiston, simultaneously with the sightingpiston of the timely washed samples of clear water, avoids at sightingpiston kish abrasive dust;
Adopt metallic phase polisher milling to sightingpiston carry out essence throwing, use woollen cloth or velveting, the metallographic lapping paste adopting granularity to be 10w and 5w with this, have noted dynamics and humidity during polishing, after polishing the sightingpiston of sample smooth, without deformation layer, no marking; With washes of absolute alcohol sample sightingpiston, confirm that erosional surface cleanliness without any pollution treated by sample.
2) clamping appropriate absorbent cotton with tweezers, dip the metallographic etchant of new preparation, take out absorbent cotton, repeatedly wiping specimen surface about 7 ~ 12min gently, is silver gray to specimen surface;
3) a certain amount of metallographic etchant of new preparation, then by step 2) sample after process immerses in the metallographic etchant of new preparation immediately, during immersion, the metallographicobservation face of sample is parallel with etching reagent liquid level, sightingpiston upwards, metallographicobservation face and erosional surface are at a distance of about 10 ~ 20mm, etch is 3 ~ 5min about, until the bubble covering specimen surface presents yellow;
4) HR-2 resistant to hydrogen steel curved beam is pressed from both sides out with tweezers, at once by the abundant washed samples of water of flowing, then draw appropriate dehydrated alcohol with glue head dropper and repeatedly rinse, electricity consumption dries up, obtain HR-2 resistant to hydrogen steel metallographic observation sample, at metallography microscope Microscopic observation corrosive effect.
Embodiment 1
An etching pit method for HR-2 resistant to hydrogen steel, concrete operations are:
Measure 25 ml distilled waters with graduated cylinder, fall in beaker, then add 15 milliliters of hydrochloric acid, finally add 5 milliliters of nitric acid, stir gently with glass stick, be mixed with metallographic etchant.
HR-2 resistant to hydrogen steel curved beam is carried out polishing and (during polishing, first roughly grinds fine grinding again, successively with the polishing of 400#, 600#, 800#, 1000# water-proof abrasive paper), mechanical polishing (10W, 5W grind), cleaning (with distilled water and washes of absolute alcohol), to dry up, make and treat corrosion sample; Clamp appropriate absorbent cotton with tweezers, dip metallographic etchant, take out absorbent cotton, wiping specimen surface is about 8min gently repeatedly, is silver gray to specimen surface; Pour the metallographic etchant of a certain amount of new preparation into small beaker, then sample is immersed in metallographic etchant, during immersion, the metallographicobservation face of sample is parallel with etching reagent liquid level, sightingpiston upwards, metallographicobservation face and erosional surface are at a distance of about 15mm, etch is about 4min, until the bubble covering specimen surface presents yellow; Press from both sides out HR-2 resistant to hydrogen steel curved beam with tweezers, at once by the abundant washed samples of water of flowing, then draw appropriate dehydrated alcohol with glue head dropper and repeatedly rinse, electricity consumption dries up, and obtains HR-2 resistant to hydrogen steel metallographic observation sample, at metallography microscope Microscopic observation corrosive effect.
As shown in Figure 2, as can be seen from the figure, original structure is single phase austenite tissue to observations, can clear display full die in figure, and the subgrain boundary of intra-die also can display.
Embodiment 2
An etching pit method for HR-2 resistant to hydrogen steel after stretched, concrete operations are:
Measure 25 ml distilled waters with graduated cylinder, fall in beaker, then add 15 milliliters of hydrochloric acid, finally add 5 milliliters of nitric acid, stir gently with glass stick, be mixed with metallographic etchant.
By deformation quantity be 10% HR-2 resistant to hydrogen steel curved beam carry out polishing (first roughly grinding fine grinding again during polishing successively with the polishing of 400#, 600#, 800#, 1000# water-proof abrasive paper), mechanical polishing (10W, 5W grind), cleaning (with distilled water and washes of absolute alcohol), dry up, make and treat corrosion sample; Clamp appropriate absorbent cotton with tweezers, dip the metallographic etchant configured by claim 2, take out absorbent cotton, wiping specimen surface is about 7min gently repeatedly, is silver gray to specimen surface; Pour a certain amount of new preparation corrosive fluid into small beaker, then sample is immersed in the corrosive fluid prepared, during immersion, the metallographicobservation face of sample is parallel with etching reagent liquid level, sightingpiston upwards, metallographicobservation face and erosional surface are at a distance of about 12mm, etch is about 5min, until the bubble covering specimen surface presents yellow; Press from both sides out HR-2 resistant to hydrogen steel curved beam with tweezers, at once by the abundant washed samples of water of flowing, then draw appropriate dehydrated alcohol with glue head dropper and repeatedly rinse, electricity consumption dries up, and obtains HR-2 resistant to hydrogen steel metallographic observation sample, at metallography microscope Microscopic observation corrosive effect.
As shown in Figure 3, as can be seen from the figure, in figure, part intra-die is due to stretching action, starts to form martensitic stucture at grain boundaries for observations, and this martensitic stucture and austenite structure can both be known by this caustic solution and manifest.
As can be seen from above two embodiments, in sample metallographic microstructure, austenite structure and strain-induced martensite organize comparison of light and shade distinct, display effect is good, surface no-pollution, the present invention can observe subgrain boundary, twin boundary, crystal boundary, austenite structure and strain-induced martensite more significantly, illustrates that the corrosive effect of metallographic etchant of the present invention to HR-2 resistant to hydrogen steel is fabulous.
Claims (10)
1. for a metallographic etchant for HR-2 resistant to hydrogen steel, it is characterized in that, the volume ratio of being pressed 1:3:5 by nitric acid, hydrochloric acid and distilled water is formulated.
2. for a compound method for the metallographic etchant of HR-2 resistant to hydrogen steel, it is characterized in that, measure nitric acid, hydrochloric acid and distilled water respectively according to the volume ratio of 1:3:5, first hydrochloric acid is dissolved in distilled water, add nitric acid again, stir, obtain the metallographic etchant for HR-2 resistant to hydrogen steel.
3. an etching pit method for HR-2 resistant to hydrogen steel, is characterized in that, comprise the following steps:
1) HR-2 resistant to hydrogen steel curved beam is carried out polish, polishing, clean and dry up process, make and treat corrosion sample;
2) absorbent cotton is dipped the metallographic etchant of new preparation, the absorbent cotton that taking-up soaks repeatedly wiping treats that corrosion sample surface to surface is silver gray;
3) by step 2) sample after process immerses in the metallographic etchant of new preparation, and the bubble that etch to specimen surface covers is in yellow; During immersion, the metallographicobservation face of sample is parallel with the liquid level of metallographic etchant, and sightingpiston upwards;
4), after being taken out by sample, through washing, drying, HR-2 resistant to hydrogen steel metallographic observation sample is obtained, at metallography microscope Microscopic observation corrosive effect;
Wherein, metallographic etchant is formulated by the volume ratio of 1:3:5 by nitric acid, hydrochloric acid and distilled water.
4. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, it is characterized in that, step 1) described in polishing be polish with the water-proof abrasive paper of 400#, 600#, 800# and 1000# successively, and every polishing together all will eliminate polishing scratch and the abrasive dust that a procedure stays metallographicobservation face.
5. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 1) described in polishing be carry out mechanical polishing with the metallographic lapping paste that granularity is 10W and 5W successively.
6. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 1) described in cleaning be clean with distilled water and dehydrated alcohol successively.
7. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 2) described in the time of wiping be repeatedly 7 ~ 12min.
8. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 3) described in the etch time be 3 ~ 5min.
9. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 3) described in metallographicobservation face and erosional surface at a distance of 10 ~ 20mm.
10. the etching pit method of a kind of HR-2 resistant to hydrogen steel according to claim 3, is characterized in that, step 4) described in washing be first use distilled water flushing, more repeatedly to rinse with dehydrated alcohol; Step 4) described in drying be with hair dryer by washing after sample dry up.
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| CN104911611A (en) * | 2015-05-05 | 2015-09-16 | 江苏省沙钢钢铁研究院有限公司 | Wiping type pickling solution for removing high-temperature alloy hot-rolled oxidation layer and application thereof |
| CN105241885A (en) * | 2015-09-30 | 2016-01-13 | 金川集团股份有限公司 | Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof |
| CN106917091A (en) * | 2017-01-11 | 2017-07-04 | 广东省工业分析检测中心 | A kind of powder of stainless steel metallographic etchant and its caustic solution |
| CN112098393A (en) * | 2020-09-14 | 2020-12-18 | 中国工程物理研究院机械制造工艺研究所 | Method for measuring multiple elements of HR-1 direct-reading spectrum of hydrogen-resistant steel pipe |
| CN113138145A (en) * | 2021-04-28 | 2021-07-20 | 辽宁忠旺集团有限公司 | Large-diameter aluminum alloy ingot casting grain size inspection device and automatic inspection method |
| CN114002221A (en) * | 2021-11-10 | 2022-02-01 | 中国航发贵州黎阳航空动力有限公司 | GH4169 alloy semi-finished product blade carbonitride display method |
| CN114295623A (en) * | 2021-12-28 | 2022-04-08 | 江苏隆达超合金股份有限公司 | Method for detecting defects of small-caliber thin-wall nickel-based high-temperature alloy pipe |
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| CN104911611A (en) * | 2015-05-05 | 2015-09-16 | 江苏省沙钢钢铁研究院有限公司 | Wiping type pickling solution for removing high-temperature alloy hot-rolled oxidation layer and application thereof |
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| CN106917091A (en) * | 2017-01-11 | 2017-07-04 | 广东省工业分析检测中心 | A kind of powder of stainless steel metallographic etchant and its caustic solution |
| CN112098393A (en) * | 2020-09-14 | 2020-12-18 | 中国工程物理研究院机械制造工艺研究所 | Method for measuring multiple elements of HR-1 direct-reading spectrum of hydrogen-resistant steel pipe |
| CN113138145A (en) * | 2021-04-28 | 2021-07-20 | 辽宁忠旺集团有限公司 | Large-diameter aluminum alloy ingot casting grain size inspection device and automatic inspection method |
| CN114002221A (en) * | 2021-11-10 | 2022-02-01 | 中国航发贵州黎阳航空动力有限公司 | GH4169 alloy semi-finished product blade carbonitride display method |
| CN114295623A (en) * | 2021-12-28 | 2022-04-08 | 江苏隆达超合金股份有限公司 | Method for detecting defects of small-caliber thin-wall nickel-based high-temperature alloy pipe |
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